Biopowered - vegetable oil and biodiesel forum
Biodiesel => Chemistry and process => Topic started by: 1958steveflying on January 20, 2013, 02:38:22 PM
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Admin addition ... There is now a wiki page to collate test results from this process see ...
http://www.biopowered.co.uk/wiki/Acetone_as_an_aid_to_transesterification
Saturday I made a 180 litre batch that had been glyc washed and venturi dried to 65c.
At 65c I added 30 litres Meth with 750g KoH and 1 litre Acetone.
My first 90/10 showed 45% unreacted and after a further 30 minutes reacting the next 90/10 showed 15% unreacted.
I settled for 30 minutes and dropped the glyc.
over the next hour I added 50g with 1 litre meth to mix then 50g then 60g to get a clear pass.
So 180 litres reacted to clear pass with 910g of KoH with 33 litres methanol and 1 litre Acetone.
After demeth I settled over night and dropped 3 litres glyc giving a total of 25 litres of glyc dropped.
The glyc dropped from stage 1 had only a tiny amount of bio in the following day whereas it would normally have about 2 inches in the cubie, so had dropped quickly and split well.
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What a result Steve
That's a base of just 5 (ish). Sounds like a very clean process too! It'll be interesting to see how much further Lye can be decreased / Acetone increased.
I'll also be interesting to see if processing temps can be lowered and by how much.
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Yes Nathan it looks good so far, next batch I shall add 2 litres Acetone, with regard to processing temperature as I followed on to dewatering it seemed daft to wait and let it cool.
At the moment its 50c and about to get pumped across and fuged as no further glyc has dropped since this morning.
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Fuge took out traces of glyc. will have to let it cool and settle and check tomorrow.
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Some good results there Steve.
I wonder if keeping reaction temps down will have a positive influence on HMPE formation.
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in the paper on using acetone, at 25% they reacted at 25c with no agitation.
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It's all very exciting... guess I need to think about building a new processor or getting mine back for a bit! Need to experiment too!
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in the paper on using acetone, at 25% they reacted at 25c with no agitation.
Yes will slowly work towards that, as I'm not recovering the Acetone for future use at the moment I shall work up on the Acetone and down on the chem's and temp. While working towards an Acetone recovery
Regarding the temp at the moment I am dewatering prior to reaction so it does not make sense not to use it.
I am thinking out loud here but if I can water test my recovered Methanol and Acetone and it is clear then I can re-use it. As my glyc is reduced I am thinking I have produced less water and therefore less soap/glyc ! due to using Acetone !
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It's all very exciting... guess I need to think about building a new processor or getting mine back for a bit! Need to experiment too!
Without re reading it, were they not using a paddle for agitation ?
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in one of the papers they are using a paddle. in the green chemistry paper, the one jules linked to they are just mixing the acetone KOH and meth with the oil at 25c and leaving for 10 minutes than draining the glys off.
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in one of the papers they are using a paddle. in the green chemistry paper, the one jules linked to they are just mixing the acetone KOH and meth with the oil at 25c and leaving for 10 minutes than draining the glys off.
Thanks I felt certain I had read use of a paddle, thought I was going mad.
I cant wait for when someone gets to just mix the the 3 components together wait for 10 mins drop glyc and the bio will be fully reacted to happen. That will be a wow moment.
We are looking at bulk purchase of Acetone this week. I will be getting a batch of oil dried ready this week too !
Working out how much KoH is the hurdle isn't it ? or has someone come across that value ?
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Working out how much KoH is the hurdle isn't it ? or has someone come across that value ?
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Steve was the lye calculation per litre of converted in the first stage match that used for unconverted in the 2nd stage?
Would be a good idea to graph the figures... We might expect to see a proportional decrease as you increase the acetone percentage. If our experience matches the research, it would taper off at 25%??
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Working out how much KoH is the hurdle isn't it ? or has someone come across that value ?
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Steve was the lye calculation per litre of converted in the first stage match that used for unconverted in the 2nd stage?
Would be a good idea to graph the figures... We might expect to see a proportional decrease as you increase the acetone percentage. If our experience matches the research, it would taper off at 25%??
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The KoH hurdle I was referring to is the amount needed for the 25c 25% Acetone reaction. I have since read that to be 0.5wt% If someone can translate that to plain English I for one would appreciate it. lol.
"calculation per litre of converted in the first stage match that used for unconverted in the 2nd stage" Not exactly, if my batch was 180 litres then the first stage worked out at 4.9g per litre and the second 5.9g per litre.
However I found exactly the same using ASM
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I'll read that research paper, see what I can glean!
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High Steve
0.5wt% if I got it right would be
100L oil x 79g per litre =79kg
79x .5% = 395 g
Think that's right just doing it in the van , will have to read more to see if this is the calc you want
Paul
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High Steve
0.5wt% if I got it right would be
100L oil x 79g per litre =79kg
79x .5% = 395 g
Think that's right just doing it in the van , will have to read more to see if this is the calc you want
Paul
Cheers Paul, so for a 180 litre batch it would work out at 711g KoH now I know what I am working towards.
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hopefully the process should work just as well with ASM. is anyone trialing that yet? if it does work as well with ASM as KOH be interesting to see what the ASM amount comes out to. of course any extra ASM shouldn't matter should it? to make it viable financially the acetone meth mix would have to be recovered so any extra meth would be got back.
i am still not sure about the best way to recover the acetone/methanol mix.i favour reduced atmosphere low temperature but not sure if just pumping the bio after the gly drop into another container and pulling a vacuum on it with a venturi as in GLs push pull system is worth the complexity.
don't know if just heating the tank and letting the condenser do all the work would work ok on its own. if that would work it would be the simplest way of doing it.
something tells me heating bio containing 36% volatiles is a bit more dangerous then the 12% or so meth in a "normal" batch of bio.
external water heating is a lot safer and doesn't have to add to much complexity to the system.
we could be jumping from home brew simple to chemical engineering complex here.
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I'm sure I read somewhere, some time ago that it was more economical to heat to remove Methanol than create a vacuum, it might have been GL.
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hopefully the process should work just as well with ASM. is anyone trialing that yet? if it does work as well with ASM as KOH be interesting to see what the ASM amount comes out to. of course any extra ASM shouldn't matter should it? to make it viable financially the acetone meth mix would have to be recovered so any extra meth would be got back.
i am still not sure about the best way to recover the acetone/methanol mix.i favour reduced atmosphere low temperature but not sure if just pumping the bio after the gly drop into another container and pulling a vacuum on it with a venturi as in GLs push pull system is worth the complexity.
don't know if just heating the tank and letting the condenser do all the work would work ok on its own. if that would work it would be the simplest way of doing it.
something tells me heating bio containing 36% volatiles is a bit more dangerous then the 12% or so meth in a "normal" batch of bio.
external water heating is a lot safer and doesn't have to add to much complexity to the system.
we could be jumping from home brew simple to chemical engineering complex here.
My reactor is twin cone water heated.. Phew ! I know I only had 1 litre Acetone and I assume it came out in the condensing process up to 90c.
No further Glyc dropped today ! ! ! previously Glyc dropped up to the 10th day so it seems not only did using the litre of Acetone in the reaction reduce the KoH needed but did in fact leave Bio that the Glyc dropped out of in 2 days.
It is bubbling now to drive off any residual Methanol and I am not able to get to it until Wed am when I will take a sample from the bottom and see what gives.
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Be aware of using a vacuum in a normal drum,
this is a photo of a 60L steel drum subjected to a venturi (so not a full vacuum).
(http://i250.photobucket.com/albums/gg264/mark405td/liamchristningmikes17th.jpg)
Notice how clean my setup is.
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i am planning to use a 47 kg N2 bottle. my problem is how do i keep the acetone out of the vacuum pump? actually i know the principle but not the practical. i know i need a cold trap but have no idea of the details of temperature or how long i need to keep it cold for. the plan is to take the valve out and fit the condenser and a tee to fill it so i don't have to make any more holes in the bottle. the vacuum pump will go on the end of the condenser. that's the plan anyway til someone comes up with a better one.
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Hi all
I will be trying a microbbatch with acetone tomorrow using my normal feedstock to see how it works for me , will also try it on some wvo using ASM.
Will try and read the info given so I can replicate it
Paul
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Hi all
I will be trying a microbbatch with acetone tomorrow using my normal feedstock to see how it works for me , will also try it on some wvo using ASM.
Will try and read the info given so I can replicate it
Paul
I'm sure many of us will look forward to the results with bated breath :)
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looking forward to the results here, btw if using acetone i pressume it can be washed out with water if not being recovered.
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looking forward to the results here, btw if using acetone i pressume it can be washed out with water if not being recovered.
i am sure you can,but its quite expensive. £1.25 per litre so 25 ltrs on a 100 litre batch is £33.00 you are flushing away plus the meth as well. i know some say the meth is not worth recovering, but the acetone certainly is.
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At 65c I added 30 litres Meth with 750g KoH and 1 litre Acetone.
Doing lots of reading :o and wondered this
Acetone boils at 56* would that not be a problem it being vapour not liquid?
Isn't that why in part in that research paper they tested at lower temps?
High Steve
0.5wt% if I got it right would be
100L oil x 79g per litre =79kg
79x .5% = 395 g
Think that's right just doing it in the van , will have to read more to see if this is the calc you want
Paul
Doesn't
100L oil x 79g per litre equal 7900g or 7.9KG ?
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something tells me heating bio containing 36% volatiles is a bit more dangerous then the 12% or so meth in a "normal" batch of bio.
12% Meth is just as likely to blow your head off if ignited ;D
Since Acetone boils at 56* and Methanol at 65* would it be possible to not only condense them off but do it in a controlled way and separate them? Isn't it called fractional distillation?
This company makes something to do this with Acetone
http://www.kcmouldings.co.uk/html/solventru.html (http://www.kcmouldings.co.uk/html/solventru.html)
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something tells me heating bio containing 36% volatiles is a bit more dangerous then the 12% or so meth in a "normal" batch of bio.
12% Meth is just as likely to blow your head off if ignited ;D
Since Acetone boils at 56* and Methanol at 65* would it be possible to not only condense them off but do it in a controlled way and separate them? Isn't it called fractional distillation?
This company makes something to do this with Acetone
http://www.kcmouldings.co.uk/html/solventru.html (http://www.kcmouldings.co.uk/html/solventru.html)
agreed 12% meths is enough to blow your head off 36% might be enough to cause some damage. ;D
that unit is really no different to a gl processor. i a planning to recover the solvent under vacuum using hot water to heat a gas bottle. have a look a acetone/methanol azeotropes. this is what we will end up with. that vapourises at 60C.
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Hi all
I didn't get a chance to do any bench work today (more problems ) all going well will have a chance tomorrow.
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have a look a acetone/methanol azeotropes. this is what we will end up with. that vapourises at 60C.
Hmmm I didn't realise they wouldn't separate easily, but do they need to be separated or can whats recovered just be reused on the next batch?
Would there be a way to know the percentage of Meth/Acetone condensed off?
Bit out of my depth so forgive any stupid suggestions :)
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have a look a acetone/methanol azeotropes. this is what we will end up with. that vapourises at 60C.
Hmmm I didn't realise they wouldn't separate easily, but do they need to be separated or can whats recovered just be reused on the next batch?
Would there be a way to know the percentage of Meth/Acetone condensed off?
Bit out of my depth so forgive any stupid suggestions :)
i know what you mean about being out of your depth.i am drowning here. experiments are the way forward. no mention of the effect of the meth on the next reaction in the paper that i can find.maybe try the trick of dropping things that are known to be affected by meth in the fuel in a jar of finished bio and wait? KH did some experiments with this a while ago. should be in the VOD archives somewhere.
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have a look a acetone/methanol azeotropes. this is what we will end up with. that vapourises at 60C.
Would there be a way to know the percentage of Meth/Acetone condensed off?
That is my concern with this as well. Meth and Acetone share very similar boil points and have very similar densities. So I'm not sure we'd be able to easily determine how much Acetone is recovered for the next process.
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have a look a acetone/methanol azeotropes. this is what we will end up with. that vapourises at 60C.
Would there be a way to know the percentage of Meth/Acetone condensed off?
That is my concern with this as well. Meth and Acetone share very similar boil points and have very similar densities. So I'm not sure we'd be able to easily determine how much Acetone is recovered for the next process.
An assumption I made from reading the original paper was that all of the Acetone was being recovered so any more volume recovered than that put in would be Methanol, just how many times you could trust this to be correct though !
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The paper says 0.02 wt% of KOH, which in a 100l batch of Rapeseed oil would be about 100*0.91*0.0002 = 18.2g. This is tiny - but then it is a catalyst...
I'm curious about the glycerol separation too, as the acetone I mixed 50:50 with my NaOH Glycerol formed a homogeneous mass which then set solid. Can someone that has KOH Glyc please repeat this?
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dont forget in the original paper they are recovering the acetone at 75 torr. according to the calculator i have that that pressure the boiling point of acetone is only 14c. they are using 60c which is quite a bit higher than the boiling point. not sure how much difference that will make but to replicate their results we should be using the same methods, at least until we have know what we are doing. of course the other way of checking it is to see how much the reaction is slowed down after recovering the acetone. if it isnt all being recovered and ending up staying in the bio the reaction should take longer. think some lab scale experiments are needed before chucking 25 ltres a of acetone into a 100 ltr mix.
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The paper says 0.02 wt% of KOH, which in a 100l batch of Rapeseed oil would be about 100*0.91*0.0002 = 18.2g. This is tiny - but then it is a catalyst...
From one of the papers
"KOH catalyst to
oil, 0.5 wt.%; temperature, 25 oC"
Are we singing from different hymn books lol.
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my hymn book in on the same page as steves. 0.1% to 0.5% wt KOH to oil.
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Just a quick one
Did micro batch 600ml
Titrated at .4 used a base of 3.5 ASM then used 75% of needed catylist
20% meth
20% acertone
Heated to 25c
Mixed for 1.5-2 mins
Got a 94% conversion
Gota go will report more later
Paul
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I know this is not directly related to the use of acetone in the reaction,
but a few years ago when I was doing single stage reactions I took samples as soon as all the methoxide had been added (took apox 3 or 4 mins),
these samples showed a suprising amount of gly had allready formed.
I tested (27/3) these and had around 80% convertion.
This was with an 80lpm pump, 22mm pipework and 180L batch, using 20% meths at 60°C.
I've posted this to put Paul test into context.
Paul has not only used less catalyst and less heat but less mixing time as well.
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Cool thanks mark
I've just mixed it up again for a couple of minuets with the Glyc still in to see if it could go to full conversion and will test it when I get back in the morning.
I think with this process we need to ask what do we want/need th achieve.
Less catylist
Less heat
Quicker mixing
From reading the papers I understand that no meth mixes in with the Glyc if this is so then there is no real reason to do wbd . This could prevent hmpe's in some cases maybe.
I talked to Steve today and he said he tried some acertone in his last batch and the Glyc settled a lot quicker but he lost about a 5th of what he would normally get
On the figures I work to that's about the volume of meth in the Glyc.
All going well I will do some more test tomorrow.
First test will be to try this at a higher temp as most react after drying so the oil is still hot , by doing this I'm hoping that we can reduce acertone and catylist and still have a quick reaction time.
Any ideas through them over and I will see what I can do.
By the way mixing acid with meth/acertone is much less volatile only just got slightly warm
That's it for a bit I'm going home
Paul
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Ah, Paul showing all the signs of running your own business (out at work past 10pm!)
Very interesting though :)
Good point on the "what do we want to achieve?".
Catalyst cost per litre is tiny, electricity approx 1-2ppl, the majority cost is Methanol which this doesn't help with.
So perhaps process time, and quality of output even with water present?
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Just quick and then I'm def going home
Another thought I had was if the Glyc doesn't consume any meth then maybe we could go down to the 12.5% required for the conversion this is something I will try and post back
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Quick summary of what I understand from this paper
http://pubs.rsc.org/en/Content/ArticleLanding/2011/GC/c1gc15049a (http://pubs.rsc.org/en/Content/ArticleLanding/2011/GC/c1gc15049a)
A few quotes
How can we accelerate the formation of FAME in the reaction
between the immiscible oil and methanol? One approach is to
accelerate the reaction by heating and another is to accelerate
it by increasing the contact interface by forming small reactant
droplets through vigorous stirring by ultrasonic irradiation.
Heat and agitation the norm for processing now.
the reaction can still only take place at the interface
between the immiscible reactants present in the heterogeneous
phases. If the FAME formation takes place in a homogeneous
phase, the reaction can be accelerated by a molecular-molecular
reaction.
In english!
immiscible = doesnt mix
heterogeneous = Diverse in character or content
homogeneous = Of the same kind; alike
So the reaction only takes place where the surfaces touch and since the reactants are different they do not mix well, a bit like globules
of oil in water. By making them mix well ie adding acetone which dissolves into the oil and FAME, the mixture allows the oil globules to
break down to a molecular level. This means there is much more surface area for the reaction to occur. ie: faster So heat and agitation is
not as important, hence lower reaction temp required.
we have concluded that the retardation of FAME formation after the
formation of GL can be explained as follows: in the case without
solvent, or with acetone or THF, GL cannot be dissolved in the
oil or FAME, but methanol and KOH catalyst dissolve well in
GL. Therefore, FAME formation is retarded after the formation
of GL due to the dissolution of the important reactant methanol
and the catalyst into the GL phase, which easily precipitates
and is excluded from the reactant solution.
So reaction slows as the methanol and KOH catalyst is taken out of the FAME in the GL(Glycerol)
Acetone does not dissolve in GL so the Acetone stays in the FAME as the GL is formed.
With acetone, which does not dissolve GL, the
separation of FAME from GL was very fast because of the
lower viscosity of the FAME-acetone solution and the large
difference between the low-density FAME-acetone solution and
GL.
Acetone rich FAME has a lower viscocity so the GL drops quicker
Therefore, in the presence of
acetone, the difference in specific gravity between FAME in
acetone (0.8395) and GL with one mole of excess methanol
(1.111) is 0.2715. Due to the large difference in specific gravity
and small viscosities of the two components, GL was rapidly
separated from the FAME solution and precipitated within
30 min.
So thats my take on it had to get it off my chest!
Opinions?
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Very useful summery, gets the old grey cell moving ... off to the shed to try some tests.
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Wormman
You got it exactly right by my understanding.
I couldn't have put it better myself.
Paul
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wormman thanks for putting it into english. you have captured the essence of what they are saying very well.
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Thanks for that :-[
As I have my arm in plaster and cannot do anything physical really not even load the dishwasher ;D I am trying to exercise the brain cells.
On the subject of recovery of Acetone/Methanol I have been looking at this:
have a look a acetone/methanol azeotropes. this is what we will end up with. that vapourises at 60C.
Would there be a way to know the percentage of Meth/Acetone condensed off?
That is my concern with this as well. Meth and Acetone share very similar boil points and have very similar densities. So I'm not sure
we'd be able to easily determine how much Acetone is recovered for the next process.
The old brain was working on this while I was sleeping and I think the key may be the Specific gravity of the liquids to identify percentages left using weight.
Specific weight of Acetone at 25*C = 0.78458
Specific weight of Methanol at 25*C = 0.78773
Therefore, Acetone has a mass of 0.78458g/mL
If we multiply this by 1000 to get a litre = 784.58g
1 litre of Methanol would weigh 787.73g
So if we take exactly 1 litre of the Acetone/Methanol mix we condense off after the reaction has finished we should be able to work out the volume of methanol in the mixture by accurate weighing. It will be mainly Acetone as the volume added was much higher to start with and the Acetone will remain in the FAME as it doesnt dissolve into the GL unlike the methanol.
I will look at the calculation method later
Brain hurts off for a rest... :o
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All very interesting, I can't wait for the results of Carrington's test!
One question that remains, how do we separate the meth from acetone when both have been condensed? Or do we even need to? can we not add them all back to the next batch?
In case of the ASM use it can mix easily back in and solid catalysts can be dissolved in sufficiently safe quantity of meth and dosed accordingly.
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One question that remains, how do we separate the meth from acetone when both have been condensed? Or do we even need to? can we not add them all back to the next batch?
In case of the ASM use it can mix easily back in and solid catalysts can be dissolved in sufficiently safe quantity of meth and dosed accordingly.
That would be the plan.
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Thanks for that :-[
As I have my arm in plaster and cannot do anything physical really not even load the dishwasher ;D I am trying to exercise the brain cells.
On the subject of recovery of Acetone/Methanol I have been looking at this:
have a look a acetone/methanol azeotropes. this is what we will end up with. that vapourises at 60C.
Would there be a way to know the percentage of Meth/Acetone condensed off?
That is my concern with this as well. Meth and Acetone share very similar boil points and have very similar densities. So I'm not sure
we'd be able to easily determine how much Acetone is recovered for the next process.
The old brain was working on this while I was sleeping and I think the key may be the Specific gravity of the liquids to identify percentages left using weight.
Specific weight of Acetone at 25*C = 0.78458
Specific weight of Methanol at 25*C = 0.78773
Therefore, Acetone has a mass of 0.78458g/mL
If we multiply this by 1000 to get a litre = 784.58g
1 litre of Methanol would weigh 787.73g
So if we take exactly 1 litre of the Acetone/Methanol mix we condense off after the reaction has finished we should be able to work out the volume of methanol in the mixture by accurate weighing. It will be mainly Acetone as the volume added was much higher to start with and the Acetone will remain in the FAME as it doesnt dissolve into the GL unlike the methanol.
I will look at the calculation method later
Brain hurts off for a rest... :o
it could as simple as mixing the condensate in some glys, if indeed we need to remove the meth from the condensate. as long as the acetone is recovered, which is the expensive solvent any meth left will just go to the next batch. most of it will be in the glys anyway so could be used for a glys wash on the next batch to keep the meth usage down. if pauls experiments show that the reaction will work with the minimun 12.5% meth needed for the reaction any extra will be a bonus.
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Based on their specific weights at 20*C
1 litre of Acetone would weigh 784.58g
1 litre of Methanol would weigh 787.73g
Additional weight for Methanol is 3.15g per litre.
So if for example 1 litre condensed distillate recovered after processing weighs say 785.30g
This would mean an additional 0.72g over the expected weight of just Acetone.
So by working out the percentage of the additional amount we can work out the volume of methanol.
eg. 0.72 divided by 3.15 = 0.2286
To get a percentage we times by 100
0.2286x100 = 22.86% and since we used 1 litre as a starting point
22.86% of 1 litre is 228.6 ml of Methanol
So we can then use this in the next batch, knowing how much Meth and how much Acetone we have in the distillate we can work out the volumes required.
I think this is right but please correct me if I am wrong I am not a chemist or mathematician! :-\
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it could as simple as mixing the condensate in some glys, if indeed we need to remove the meth from the condensate. as long as the acetone is recovered, which is the expensive solvent any meth left will just go to the next batch. most of it will be in the glys anyway so could be used for a glys wash on the next batch to keep the meth usage down. if pauls experiments show that the reaction will work with the minimun 12.5% meth needed for the reaction any extra will be a bonus.
I think that is a pretty simple way actually just allow glys to settle and the acetone would be on top :)
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it could as simple as mixing the condensate in some glys, if indeed we need to remove the meth from the condensate. as long as the acetone is recovered, which is the expensive solvent any meth left will just go to the next batch. most of it will be in the glys anyway so could be used for a glys wash on the next batch to keep the meth usage down. if pauls experiments show that the reaction will work with the minimun 12.5% meth needed for the reaction any extra will be a bonus.
I think that is a pretty simple way actually just allow glys to settle and the acetone would be on top :)
Mmmmmm, but the Acetone could still contain Methanol, the Glyc does not have any properties over the Acetone to attract the Methanol.
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Just a quick one
Also in the distillate will be a % of water so not sure how accurate a sg test would be.
I could do a water in oil test but using a meth/water / acertone to see if I can get a accurate water result then do some simple sg test to see how well the calc's work out.
I'm affraid this my be a test for another day
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it could as simple as mixing the condensate in some glys, if indeed we need to remove the meth from the condensate. as long as the acetone is recovered, which is the expensive solvent any meth left will just go to the next batch. most of it will be in the glys anyway so could be used for a glys wash on the next batch to keep the meth usage down. if pauls experiments show that the reaction will work with the minimun 12.5% meth needed for the reaction any extra will be a bonus.
I think that is a pretty simple way actually just allow glys to settle and the acetone would be on top :)
Mmmmmm, but the Acetone could still contain Methanol, the Glyc does not have any properties over the Acetone to attract the Methanol.
a bit of extra meth wont matter as long as it is not in the finished bio. any left in the bio could be bubbled off. not sure how you would test for meths left in the bio. i am sure there is a simple test for this but i would have to a lot of backtracking to remember what it is. this is where the more experienced brewers could help as i am sure it has come up at at sometime.
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it could as simple as mixing the condensate in some glys, if indeed we need to remove the meth from the condensate. as long as the acetone is recovered, which is the expensive solvent any meth left will just go to the next batch. most of it will be in the glys anyway so could be used for a glys wash on the next batch to keep the meth usage down. if pauls experiments show that the reaction will work with the minimun 12.5% meth needed for the reaction any extra will be a bonus.
I think that is a pretty simple way actually just allow glys to settle and the acetone would be on top :)
Mmmmmm, but the Acetone could still contain Methanol, the Glyc does not have any properties over the Acetone to attract the Methanol.
a bit of extra meth wont matter as long as it is not in the finished bio. any left in the bio could be bubbled off. not sure how you would test for meths left in the bio. i am sure there is a simple test for this but i would have to a lot of backtracking to remember what it is. this is where the more experienced brewers could help as i am sure it has come up at at sometime.
Modified alcohol breath testers can be used to test for residual Meth in the Bio.
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Just a quick one
Also in the distillate will be a % of water so not sure how accurate a sg test would be.
I could do a water in oil test but using a meth/water / acertone to see if I can get a accurate water result then do some simple sg test to see how well the calc's work out.
I'm affraid this my be a test for another day
That would be good thanks, narrowing everything down :)
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Just a quick one
Also in the distillate will be a % of water so not sure how accurate a sg test would be.
I could do a water in oil test but using a meth/water / acertone to see if I can get a accurate water result then do some simple sg test to see how well the calc's work out.
I'm affraid this my be a test for another day
Also When meths is condensed off normally is there a level of water in that then I thought it was pure?
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Reclaimed meth always contains some water. I get mine comes in at about 96% which is fine for me.
I was talking to someone this week who gets it back at 99.8% but his colum cost 400k so I'm happy with 96%
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it could as simple as mixing the condensate in some glys, if indeed we need to remove the meth from the condensate. as long as the acetone is recovered, which is the expensive solvent any meth left will just go to the next batch. most of it will be in the glys anyway so could be used for a glys wash on the next batch to keep the meth usage down. if pauls experiments show that the reaction will work with the minimun 12.5% meth needed for the reaction any extra will be a bonus.
I think that is a pretty simple way actually just allow glys to settle and the acetone would be on top :)
Mmmmmm, but the Acetone could still contain Methanol, the Glyc does not have any properties over the Acetone to attract the Methanol.
a bit of extra meth wont matter as long as it is not in the finished bio. any left in the bio could be bubbled off. not sure how you would test for meths left in the bio. i am sure there is a simple test for this but i would have to a lot of backtracking to remember what it is. this is where the more experienced brewers could help as i am sure it has come up at at sometime.
Modified alcohol breath testers can be used to test for residual Meth in the Bio.
[/quote
just had a quick google,and it looks as if potassium dichromate will detect methanol by turning it in formic acid which you can smell. not sure about the breathtesters. are they multi use or single shot?
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Multi use, Nathan Has one we are yet to try with fully demethed Bio.
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Having read thewormman's summery earlier today it set me thinking ...
The main action of Acetone is to aid intimate mixing of the oil and Methanol. This works because Acetone is miscible with both oil and Methanol.
Biodiesel is also miscible with both oil and methanol, probably not as well, but it's available to us at minimal cost and it won't need removing from the process.
I've done a quick test. Nothing scientific just jars of new sunflower oil, very roughly 20% Methanol and a "splash" of Biodiesel.
Gave the mixes a gentle end over end shake in the shed ambient of around 8°C and there was a noticeable difference between the jars with Bio and the control without. No catalyst was included.
Jars were taken inside and sat on a radiator for half an hour and gently shaken again. This is the result ...
(http://www.palmergroup.co.uk/Bio/Methanol-oil-bio.JPG)
From left to right ... Oil and Methanol only, Oil + a Methanol and Bio mix (gently shaken), Oil and Bio mix (gently shaken) + Methanol.
Anyone any thoughts? Can someone replicate the experiment to make sure I'm not being a complete Muppet?
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Multi use, Nathan Has one we are yet to try with fully demethed Bio.
Did he give you the acid?
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Can't see the pick's
Could see the ones from yesterday
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The ones yesterday were uploaded to the wiki because I was going to add them to the Dr Pepper page.
I'll stick this one on the wiki too, it's currently on my web space.
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There you go ...
(http://www.biopowered.co.uk/w/images/0/06/Methanol-oil-bio.JPG)
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Hi Julian
I can see your workings but I'm not sure we could introduce enough catylist into the mix using bio as a cosolvent . Really nice idea tbough
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My thoughts were to use the normal methanol quantity with ASM and enough bio to help mix. Why would bio impede catalyst addition?
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Hi Julian
I'm not sure but if you used the same amount of bio as you do meth then and you put the right amount of catylist in you would be massively overdosing the bio but it may just work . Think reaction temp wants to be up in the 60's to help it all on .
I could make it my first test in the morning . If it goes ok we can work out which way we want to go.
Lower temp
Faster reaction
Less chem's
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This thread has grown very quickly today, guess I'm the only one that's been to work.
Dave (thewormman).
Considering you've yet to make any bio you've really got a good understanding of the principles involved.
When I said to do some reading I didn't expect you to learn so much so quick, well done mate,
sounds like you're going to be a valued member on here.
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Julian
I am missing something. If the bio is a good co solvent then I would have thought that as soon as a reaction started, in a normal reaction, and bio was made this would accelerate the process and the reaction would then compleat quickly?
Dick
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Julian
I am missing something. If the bio is a good co solvent then I would have thought that as soon as a reaction started, in a normal reaction, and bio was made this would accelerate the process and the reaction would then compleat quickly?
Dick
I'd tend to agree but as far as I can see the bio is doing a very similar thing to the Acetone. What helped this train of thought was to see the changes in colour and consistency when I did the Dr Pepper test the other day. See photos in this thread ... http://www.biopowered.co.uk/forum/index.php/topic,874.0/topicseen.html.
I just wish I understood the chemistry of all this even to a minor degree, but anything is worth a try.
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If anybody needs some Acetone for future experiments my supplier has 2 x 25lt left at the old price. They are £30 each. Not a bad price I'm told. I'm sure someone somewhere can get it cheaper but that's the current price I can get it for.
I'm picking a 25lt up for photoman tomorrow. I could easily pick up the other two.
Trying to help ;)
Nige
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One thought with the bio cosolvent theory
The acertone prevents the meth being drawn into the Glyc this helps keep the max amount of meth for the conversion but if using bio as the cosolvent then the meth can be consumed by the Glyc this making the reaction slower
Will still give it a go in the morning and post results
Will also post up on yesterday's micro batch after it was mixed a second time for 1.5 mins at 20c with the Glyc left in.
All looking good and interesting
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A couple of hours ago I added 3ml of neat ASM to the sample that looked the most homogeneous ... the one where I mixed the Methanol and Bio together before adding to the oil. This has been shaken gently and left on a radiator. I guess the temperature of the sample is around 20°C.
This is what it looks like ...
(http://www.biopowered.co.uk/w/images/8/85/Methanol-oil-bio_and_ASM.JPG)
It's certainly changed, into what I don't know. The answer to the obvious question is no, there's no drop out of any sort!
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It looks good but ----- try a 10/90 as a starting point.
Dick
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Good idea, I don't suppose for one minute it will show anything but 100% drop out, but I'll give it a go tomorrow.
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I have no idea of the normal asm per liter dose, so I'll ask, should 3ml be enough to fully convert that amount of fresh oil ?
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I have no idea of the normal asm per liter dose, so I'll ask, should 3ml be enough to fully convert that amount of fresh oil ?
You want me to do sums at this time of night?
I've no idea, I just lobbed some in with a pipette.
You've got me thinking now, what's the volume of a jam jar?
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There was me thinking you'd calculated the volumes to do a propper scientific test.
I should have known better.
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Scientific ... just remind me what that is again.
Just had a look and I'd guess at 400ml so the samples are probably around 200ml.
With a base of 3.5 that would require ... 0.2 x 3.5 x 5 = 3.5ml. So it's close.
Oh and I cant make Tuesday morning next week now ... had a call from a school with 200 ltrs of oil they won't take payment for.
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Three hours on there's just a faint sign of glycerine forming at the bottom of the jar. The heating has gone off so the sample is cooling a little.
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I am thinking of adding acetone to a NaOH batch tomorrow.
Am I correct in thinking that if acetone is used then the glyc does not take up meth?
This being the case how quickly does the glyc set if NaOH is used?
Opinions please.
Dick
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Hi dick
Yes your right the Glyc should not take up any meth so I think it will be a temperature thing as to how quick the Glyc goes solid.
It should drop much faster so will still be hot when the majority of the Glyc has settled.
Paul
I will see if the Glyc has set in the sample batch using asm
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That confirms my thinking.
If using NaOH it will be difficult to react at low temperature as there is a substantial risk of the glyc setting in the pipe work. It may be time to experiment with a continuous glyc extraction system.
Dick
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Yes your right the Glyc should not take up any meth
Hi could you explain why that is or point me at something I can read about it?
Thanks :)
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This thread has grown very quickly today, guess I'm the only one that's been to work.
Dave (thewormman).
Considering you've yet to make any bio you've really got a good understanding of the principles involved.
When I said to do some reading I didn't expect you to learn so much so quick, well done mate,
sounds like you're going to be a valued member on here.
Cheers Mark Been reading masses so I dont try and do something physical :)
Good news is plaster came off yesterday and doc said didnt need a caliper ;D I can straighten it carefully and drive in a week!!!
Cant lift with it though for 10 weeks, dont need to lift to wire my processor though, gonna start next week ;D
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Good news is plaster came off yesterday and doc said didnt need a caliper ;D I can straighten it carefully and drive in a week!!!
Cant lift with it though for 10 weeks, dont need to lift to wire my processor though, gonna start next week ;D
That's good news mate, just take things slowly, you don't want to over do it and cause problems later.
That said, I'd find it very hard not to do stuff, it's just not in my nature.
I've been slowly emptying out my shed ready for the big reactor tank that's coming soon,
280L of gly gone allready.
Still can't put a mug down though.
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Hi all
Bad day today, back went out last night so lots of pain today so didn't realy do much in the way of samples but did check the micro batch from the other day.
600ml batch mixed at 25c with
20%meth
20%acretone
75% ASM
Mixed for 1.5-2 mins
94% conversion
Left to settle for few hours
Then mixed with glyc still in
Checked today and have .05ml dropout
So still looking good
Paul
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Paul
What do you think about getting Ben to test a fully finished sample that's been produced using acetone as a co-solvent?
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Not very scientific but I did a Dr Pepper. 1L oil at 30c 200ml meth with 4 .5g NaOH dissolved in it. the left hand bottle had 100ml acetone. shook both for 30 seconds then left. The acetone started to react quicker but not appreciably so.
left overnight in a warm place.
The results are below
(http://i1279.photobucket.com/albums/y521/dickjotec/90467058c0a78dcfb12ae6137f2e4ecc_zps036b5d10.jpg)
As I hope you can see the acetone has produced less glyc and a better conversion.
I am now demething a 160L batch which has had less chemicals than normal 1.6 L acetone and the first settle produced half the usual a amount of meth with a drop out of 3.
Will report after it has completed.
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I have completed a batch using acetone and while it could just be an unusual batch I am very impressed.
Normal 2 stage for me.
Dry oil by heating and settling. 160L in processor.
Stage 1
30l meth 5.5 base 900g NaOH
1hour mix
Stage 2
Fallout typically 3 so about 280g
Meth about 9L
About 35L of glyc and 145L bio and 14L reclaimed meth WBD
Today
25L meth. 800 NaOH
1.5L acetone
Fallout 1.5
5L meth 130g NaOH
Good pass
Glyc 25L bio 160L meth reclaimed 8L just from bio.
So 10+ L less glyc 15+L more bio. Next time I will cut the chemicals down more and then start adjusting the times. Very impressed so far.
The glyc has not set yet and I suspect that there is meth in it. Next time I will WBD.
Dick
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I have completed a batch using acetone and while it could just be an unusual batch I am very impressed.
Today
25L meth. 800 NaOH
1.5L acetone
Fallout 1.5
5L meth 130g NaOH
Good pass
Glyc 25L bio 160L meth reclaimed 8L just from bio.
So 10+ L less glyc 15+L more bio. Next time I will cut the chemicals down more and then start adjusting the times. Very impressed so far.
The glyc has not set yet and I suspect that there is meth in it. Next time I will WBD.
Dick
That looks a good result Dick, nice one.
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Hi dick
Could do a test with the Glyc and warm it up in a glass jar to see if vapours come of (could be meth ).
The use of acetone should prevent the meth going into the Glyc , if this is so then we could definitely use les meth as well as catalyst.
I think this is why we're getting less Glyc as it contains much less meth
Paul
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Hi Paul,
Will give it a go tomorrow.
ATM I am thinking that the acetone may well stop the meth going into the glyc when acetone is used at high percentages, eg 25%, but it is still in there at low percentages, eg 1%, which is what I used.
Dick
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I've just finished a full 3.5k batch with only 3L of acetone and had fantastic results with reaction time and also 1stage to completion (would normally need 2stage )
Going to do some test using 13% meth to see how it goes
Paul
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Very interesting less than .1% acetone makes a significant improvement. Have you tested your glyc?
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Not till the morning . Supprisingly the Glyc in the sample a took settled much quicker and also much clearer than normal leading me to believe the sg diference of both products is greater than normal so will also be testing sg of Glyc as well.
Sorry edited to make more sence
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The glyc from mine was clearer as well, not as black, almost like a thicker dark bio.
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The glycerine phase of the Glyc by-product is light honey coloured
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Correct me if I'm wrong, but surely the increase of bio is due to the meths stying in the bio not the gly.
This could be checked by demething both bio and gly, them measuring the bio, gly and the, well lets refer to it as condensate as we don't know the concentration of meths to acetone.
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Correct me if I'm wrong, but surely the increase of bio is due to the meths stying in the bio not the gly.
This could be checked by demething both bio and gly, them measuring the bio, gly and the, well lets refer to it as condensate as we don't know the concentration of meths to acetone.
I demethed for the usual amount of time and only got 8L where I would normally get 12+ so I don't think it is in the bio. Next batch in 3 weeks I will WBD Which will answer if it is in the glyc.
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Yes I think you are right mark
If this is the case then if we can get the meth down to 13ish% then the condensate should be mostly acetone hopefully.
I think there's lots of work till we get it perfected but just knowing that a small amount makes a good difference means that most test done using acetone should be beneficial.
Going on results so far i think we can say that we can reduce the quantity that's reported in the research paper.
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Yes I think you are right mark
If this is the case then if we can get the meth down to 13ish% then the condensate should be mostly acetone hopefully.
I think there's lots of work till we get it perfected but just knowing that a small amount makes a good difference means that most test done using acetone should be beneficial.
Going on results so far i think we can say that we can reduce the quantity that's reported in the research paper.
I think it will be a trade between Acetone and reaction temperature.
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I think that as most people dry oil first then react i don't think temp is a issue , if we can get the meth/ catalyst down and speed up reaction then that would be a good use of the acetone.
Maybe we could work out the different quantities required for each improvement so people could choose which way they wanted to go
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Ok so it it does prove to be an increase in yield, decrease in gly, this (to me) seems to be the biggest benefit.
Now it's been reported that ASM has a similar effect (some say more bio out than veg in), so with this in mind,
I wonder if the ideal process could well be,
Gly wash to reduce FFA's,
two stage non titration with ASM + acetone (to reduce the amount of catalyst and meth),
WBD to reclaim the acetone and meths (should this be acid titration to reduce HMPE formation, would this effect the meth/acetone purity?),
pump water washing with acetone.
Yes I know it's getting complicated, but if there's a possibility of better conversions with less meth/catalyst used and reduced costs, plus a better yield it could be worth the effort.
Sadly I'm in position to do any testing on this.
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Hi mark
The acid shouldn't distill out with the meth/ acetone so Purity of distillate shouldn't be a problem.
I'm still not sure about wbd I think if there is meth left in Glyc then it would be better to take advantage of it with the Glyc wash.
Yes I think you a right about the effort if we get it right now things could get really easy in the future
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Mark
I have the dry powdered acid , if you want some I will get some down to you
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So you also see the advantage of this method, I wasn't sure I'd grasped all the information correctly.
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Mark
I have the dry powdered acid , if you want some I will get some down to you
That would be great mate, I've been waiting for some sulphuric before I can test the WBD with acid.
That said I want to finish the testing on water washing with acetone before I start changing things.
Also I don't use ASM so can't follow up on my thoughts.
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The use of acetone should prevent the meth going into the Glyc , if this is so then we could definitely use les meth as well as catalyst.
I think this is why we're getting less Glyc as it contains much less meth
Paul
Why do you think this?
There is nothing in the research that says this so could you point me at whatever states this?
Methanol readily dissolves into Glyc Acetone doesn't, Meth and Acetone do not form a compound but stay separate.
Thanks
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The use of acetone should prevent the meth going into the Glyc , if this is so then we could definitely use les meth as well as catalyst.
I think this is why we're getting less Glyc as it contains much less meth
Paul
Why do you think this?
There is nothing in the research that says this so could you point me at whatever states this?
Methanol readily dissolves into Glyc Acetone doesn't, Meth and Acetone do not form a compound but stay separate.
Thanks
Hi Dave
In the papers that I have I'm sure it list the different cosolvents used and there different properties and the reason that acetone worked better than others (ipa and xylene ) was the it doesn't mix with glycerine but the others do . If you send me your email I will send over the papers I have.
Paul
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I have just tested the glyc from yesterday by heating.
Heated with a blowtorch from below.
Fumes given off and surface flames.
Old demethed glyc just boils.
So it sounds like it does have meth in it. It has also not set overnight which also tends to suggest there is meth in it. Next batch I will WBD and see how much comes back.
Dick
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The use of acetone should prevent the meth going into the Glyc , if this is so then we could definitely use les meth as well as catalyst.
I think this is why we're getting less Glyc as it contains much less meth
Paul
Why do you think this?
There is nothing in the research that says this so could you point me at whatever states this?
Methanol readily dissolves into Glyc Acetone doesn't, Meth and Acetone do not form a compound but stay separate.
Thanks
Hi Dave
In the papers that I have I'm sure it list the different cosolvents used and there different properties and the reason that acetone worked better than others (ipa and xylene ) was the it doesn't mix with glycerine but the others do . If you send me your email I will send over the papers I have.
Paul
I think you have just made the point that the Acetone does not mix with the Glycerine Paul, I have not found anything saying the Methanol does not mix with it, have been looking back through since you said. I will stand corrected though as I can easily misread these days. lol.
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I have just tested the glyc from yesterday by heating.
Heated with a blowtorch from below.
Fumes given off and surface flames.
Old demethed glyc just boils.
So it sounds like it does have meth in it. It has also not set overnight which also tends to suggest there is meth in it. Next batch I will WBD and see how much comes back.
Dick
It may be that it only prevents the meth/Glyc mixing with a higher dose of acetone . When my codeine where's of I will be trying a micro batch using 13% meth and = amount of acetone . Will then test the Glyc
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Next batch I will WBD and see how much comes back.
Dick
Is WBD still considered best practice?
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i feel it is important to follow the experimental method in the paper as closely as possible otherwise we will get confusing results. ok recovering the acetone at 25 torr might prove a bit difficult, but that doesn't affect the reaction. once we have established a base line then is the time to experiment with less acetone. being as non of us are trained chemists, as far as i know? it is important if a chemist did come along to present them with the same experiment as in the paper.
i know i am struggling with a lack of basic chemistry. if they used 25% acetone there must have been a good reason. if it worked with 10% i am sure that is what they would have used and if they did they would have said.
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Hi all just a quick one
I think I have got something wrong with regards to meth not being consumed by Glyc when acetone is mixed with it
On first reading I understood it that as acetone is immiscible with Glyc the I took it that so would the meth be when mixed with acetone. Lao the few results we have had in defiantly produced less Glyc by about 20% and this amount is what I'd expect to find in the Glyc I use , so I'm sorry to say I put 2n2 together and believed that my assumption was right .
Wormman asked me about this as he couldn't find any info to back this up , so I have go over the papers again (a few times) and he is right ,
Also dick tested his Glyc for meth and it proved positive for meth.
Sorry that I got it wrong and led people to believe a inaccuracies and thanks to Dave for getting me to look over it again
Just proves lots more testing to be done
Paul
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i feel it is important to follow the experimental method in the paper as closely as possible otherwise we will get confusing results. ok recovering the acetone at 25 torr might prove a bit difficult, but that doesn't affect the reaction. once we have established a base line then is the time to experiment with less acetone. being as non of us are trained chemists, as far as i know? it is important if a chemist did come along to present them with the same experiment as in the paper.
i know i am struggling with a lack of basic chemistry. if they used 25% acetone there must have been a good reason. if it worked with 10% i am sure that is what they would have used and if they did they would have said.
I cant say I am in agreement with you on this, we know it works with the amounts they used, they have written the paper. However for me it is impracticable to use these amounts without the ability to recover the Acetone in a guaranteed re-usable state. We know why and how it works and using as little as 1 litre in a 180 litre batch had positive results based on our usual 2 stage no titration method. My next batch will have more adjustments which will either further improve my previous results or not.
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Paul I will always question things to find a definitive answer if I cannot see it myself, I am not trying to find fault, but just not making assumptions. I think it comes from years of working on things that could injure people if what I did was wrong.
I have also learnt over the years of losing a few jobs that I need to accept I make errors too, so I now accept graciously if they are pointed out to me :) that one took a while...
We are all human and I find the best way to get the best results is to crosscheck everything.
Just a quick one
Also in the distillate will be a % of water so not sure how accurate a sg test would be.
I could do a water in oil test but using a meth/water / acertone to see if I can get a accurate water result then do some simple sg test to see how well the calc's work out.
I'm affraid this my be a test for another day
Did you manage to do this test? I really would like to find a way of identifying Meth/Acetone percentages in the distilate. I think if we can find this then a high percentage of the Acetone can be recovered and since it is not actually consumed during the reaction the volume used is academic. We can just use the optimum 25% or whatever is best.
Dave
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Did you manage to do this test? I really would like to find a way of identifying Meth/Acetone percentages in the distilate. I think if we can find this then a high percentage of the Acetone can be recovered and since it is not actually consumed during the reaction the volume used is academic. We can just use the optimum 25% or whatever is best.
Dave
i have had a quick look at using chromatography to check to pecentages of meth and acetone. checking if you have any meth left can be done using potassium di chromate mixed with battery acid. it changes colour in the presence of methanol.
having also spent years designing and using things that can kill people i also like to know what i am doing before i do it.
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i feel it is important to follow the experimental method in the paper as closely as possible otherwise we will get confusing results. ok recovering the acetone at 25 torr might prove a bit difficult, but that doesn't affect the reaction. once we have established a base line then is the time to experiment with less acetone. being as non of us are trained chemists, as far as i know? it is important if a chemist did come along to present them with the same experiment as in the paper.
i know i am struggling with a lack of basic chemistry. if they used 25% acetone there must have been a good reason. if it worked with 10% i am sure that is what they would have used and if they did they would have said.
I cant say I am in agreement with you on this, we know it works with the amounts they used, they have written the paper. However for me it is impracticable to use these amounts without the ability to recover the Acetone in a guaranteed re-usable state. We know why and how it works and using as little as 1 litre in a 180 litre batch had positive results based on our usual 2 stage no titration method. My next batch will have more adjustments which will either further improve my previous results or not.
agreed we know it works according to the paper. but what the paper doesn't say is if it will work as well will smaller quantities of acetone. how much meth is taken up by the GL may well vary using different percentages of acetone. what i mean by this is we may be assuming the relation in linear. it may be or it may not be. unless we test using the same ratio we wont know. i don't see why it shouldn't be linear but i can't say that for certain until it is tested. not wanting to waste acetone because it might not all be recovered is not a very scientific approach in my humble opinion. there might be a magic percentage but all we know is 25% seems to be the maximun.
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i feel it is important to follow the experimental method in the paper as closely as possible otherwise we will get confusing results. ok recovering the acetone at 25 torr might prove a bit difficult, but that doesn't affect the reaction. once we have established a base line then is the time to experiment with less acetone. being as non of us are trained chemists, as far as i know? it is important if a chemist did come along to present them with the same experiment as in the paper.
i know i am struggling with a lack of basic chemistry. if they used 25% acetone there must have been a good reason. if it worked with 10% i am sure that is what they would have used and if they did they would have said.
I cant say I am in agreement with you on this, we know it works with the amounts they used, they have written the paper. However for me it is impracticable to use these amounts without the ability to recover the Acetone in a guaranteed re-usable state. We know why and how it works and using as little as 1 litre in a 180 litre batch had positive results based on our usual 2 stage no titration method. My next batch will have more adjustments which will either further improve my previous results or not.
agreed we know it works according to the paper. but what the paper doesn't say is if it will work as well will smaller quantities of acetone. how much meth is taken up by the GL may well vary using different percentages of acetone. what i mean by this is we may be assuming the relation in linear. it may be or it may not be. unless we test using the same ratio we wont know. i don't see why it shouldn't be linear but i can't say that for certain until it is tested. not wanting to waste acetone because it might not all be recovered is not a very scientific approach in my humble opinion. there might be a magic percentage but all we know is 25% seems to be the maximun.
I am not nor ever will be a scientist so doubt I will ever take a scientific approach, time to go underground I think.
dont do that!! my comments are not directed to anyone in particular. just trying to establish some scientific method to the process. your experiments are what got us here in the first place. please carry on reporting your results.
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Acetone is definitely miscible with NaOH Glyc, and it rapidly sets solid (50:50 ratio) without any separation. This is in the absence of Methanol, however.
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Acetone is definitely miscible with NaOH Glyc, and it rapidly sets solid (50:50 ratio) without any separation. This is in the absence of Methanol, however.
That was an interesting finding of your's Tony I will try a sample of KoH glyc and Acetone.
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Acetone is definitely miscible with NaOH Glyc, and it rapidly sets solid (50:50 ratio) without any separation. This is in the absence of Methanol, however.
Do they separate when heated and liquid again?
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Acetone is definitely miscible with NaOH Glyc, and it rapidly sets solid (50:50 ratio) without any separation. This is in the absence of Methanol, however.
Do they separate when heated and liquid again?
Not tried this though I need to in order to get the solid lump out of Nathanrobos nice centrifuge glassware :-\
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I have just finished the bubbling of the bio I made on Saturday. It has had 24 hours bubbling.
On the surface is a thick sheet of thick foam, it looks like HPME. I have never had this before could just be coincidence or could be the acetone? Will take a pic and test it later. If it is HPME I wonder how much more is in the tank?
Dick
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Hi Dick I almost always get it, it depends how long I bubble for. 24 hours is usually not enough for it to form, but if bubbled longer (36 hours) it will almost always appear. I assumed it was soaps and its presence was an indication that all the Methanol was successfully removed. I give it a good stir into the surface liquid and it sinks to the bottom.
If it is soaps, then maybe Acetone has somehow reduced the Methanol content in some way?
If it's HMPEs then that raises a bunch of other questions!
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I have just finished the bubbling of the bio I made on Saturday. It has had 24 hours bubbling.
On the surface is a thick sheet of thick foam, it looks like HPME. I have never had this before could just be coincidence or could be the acetone? Will take a pic and test it later. If it is HPME I wonder how much more is in the tank?
Dick
I had that once when my bubble stone was really low in the tank, I made the assumption it was stirring up the soaps that were trying to settle,
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The sample I did last at the weekend has been left to settle and now has a layer if crust on the top, this sample was
25%meth
25% acetone
75% required ASM using a base of 3.5
Mixed twice but Glyc left in between mixing
1st mix 1.5-2 mins
2nd mix 2mins
Temp 25c
Will see if I can test it
Paul
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I have just finished the bubbling of the bio I made on Saturday. It has had 24 hours bubbling.
On the surface is a thick sheet of thick foam, it looks like HPME. I have never had this before could just be coincidence or could be the acetone? Will take a pic and test it later. If it is HPME I wonder how much more is in the tank?
Dick
I had that once when my bubble stone was really low in the tank, I made the assumption it was stirring up the soaps that were trying to settle,
You could be right. I used a new bubbler as the normal one fell off the pump into the bio! The new one is longer.
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It looks like the foam is HMPE
(http://i1279.photobucket.com/albums/y521/dickjotec/9e0ef28a4866d0c9a7f04d2536c38f74_zpsf82d87ab.jpg)
Foam
I have heated a sample to 50C and it is clear. A mix with 50/50 water is now splitting, it is in a hot45C room.
(http://i1279.photobucket.com/albums/y521/dickjotec/5e5699f724724a81f3a78433adc52386_zpsf363a3c0.jpg)
Hot sample on left initial water mix on right.
Have taken a sample from the bottom of the tank and the bio is cloudy but has no evidence of 'cotton wool'. It is settling and showing clear bio above HMPE.
Perhaps the acetone stops HMPEs coalescing?
Dick
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It looks like the foam is HMPE
(http://i1279.photobucket.com/albums/y521/dickjotec/9e0ef28a4866d0c9a7f04d2536c38f74_zpsf82d87ab.jpg)
Foam
I have heated a sample to 50C and it is clear. A mix with 50/50 water is now splitting, it is in a hot45C room.
(http://i1279.photobucket.com/albums/y521/dickjotec/5e5699f724724a81f3a78433adc52386_zpsf363a3c0.jpg)
Hot sample on left initial water mix on right.
Have taken a sample from the bottom of the tank and the bio is cloudy but has no evidence of 'cotton wool'. It is settling and showing clear bio above HMPE.
Perhaps the acetone stops HMPEs coalescing?
Dick
I have done a 50/50 test on my settled batch and have a heavy white line in between water and Bio. I have fuged a fair amount of HMPE/wax out already so yet to work out what this is, I am going to have to try some acid neutralisation samples maybe.
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BTW the glyc from the batch on Saturday has now set. I will do a 50/50 tomorrow and see what the interface is like.
Dick
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I meant to add that your beer head picture looks exactly like mine did when the bubbler was too low, that was before I ever added Acetone to anything other than my fuel tank.
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I'll keep that in mind and lift it next batch but I think you said yours was soap? I am sure this is HMPE but it could be lifted from the bottom in the air like the soap. The soap in the bottom of my tank is almost always a solid which I have to dig out.
Dick
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I meant to add that your beer head picture looks exactly like mine did when the bubbler was too low, that was before I ever added Acetone to anything other than my fuel tank.
Same here with my bubbling for a long time (also a low bubbler - never even thought that height would affect it - next batch it'll be higher to see what happens).
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I'll keep that in mind and lift it next batch but I think you said yours was soap? I am sure this is HMPE but it could be lifted from the bottom in the air like the soap. The soap in the bottom of my tank is almost always a solid which I have to dig out.
Dick
Sorry that was an assumption of mine, I think I scooped it out and it ended up being discarded without any testing at all.
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I usually keep my bubbler quite a distance from the bottom of the drum. It's surprising how much of a circulation it can set up.
Similar theory to an air lift pump I think, although I suspect liquid density may come into play in the diagram ...
(http://www.fao.org/docrep/010/ah810e/AH810E119.gif)
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My bubblier was always in the very bottom, I'd have to pull it out of the settled soap/gly each time I did a new batch,
and then let it rest on top.
I've only ever seen honeycomb looking stuff form on top, and this was if I'd made a really soapy batch.
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My bubblier was always in the very bottom, I'd have to pull it out of the settled soap/gly each time I did a new batch,
and then let it rest on top.
I've only ever seen honeycomb looking stuff form on top, and this was if I'd made a really soapy batch.
My bubbler is also resting on the last batches drop out and I never get a head like that in the picture. I did in the very early days of bio brewing but not for years now.
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Jim, what did you put the head down to? I have never had one till this batch with the acetone.
Dick
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Jim, what did you put the head down to? I have never had one till this batch with the acetone.
Dick
Wet feedstock and/or excess of catalyst are the main suspects.
I'm getting some Acetone soon and will be playing with a few of my own ideas namely ASM and AAF reaction and distillation via the RED.
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Oil was as dry or drier than normal and it was the least catalyst I have ever used for a full reaction so that rules those two out. Btw what is RED?
Dick
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Btw what is RED?
Dick
Ah, that's the new name for a Squirrel, a Rapid Evaporation Devise or Red Squirrel
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Is it the same as the 'old' squirrel or a new device or just another new acronym?
I shall be interested to read your experiments with acetone, it seems like a big step forwards, too good to be true! Perhaps like all TGTBT it is not true?
Dick
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Hi all
Tomorrow I'm going to some test on the Glyc produced from acrtone reaction I'm wondering if the soaps and catylist remain more so in the bio than in the Glyc.
Maybe this is why we're seeing less Glyc
If this is so then it could cause some problems with de mething alone
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Hi all
Tomorrow I'm going to some test on the Glyc produced from acrtone reaction I'm wondering if the soaps and catylist remain more so in the bio than in the Glyc.
Maybe this is why we're seeing less Glyc
If this is so then it could cause some problems with de mething alone
That would explain the seemly higher yield, and Dick's foamy top.
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Yes the is some strange stuff going on.
With my micro batch 13% meth/Glyc. 75% catylist
Heavy layer of soap between Glyc / bio
Crust over the top of bio that I believe to be hmpe
My first batch 20% meth/Glyc
Decanted from Glyc
Heavy formation of soap through the whole sample
Steve also has a anomalies that we're going to look at today.
IMHO I think that we should probably hold back on full batches for a few days till we get the cleanup sorted.
Paul
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What was the 3k batch like? That only had .01% acetone IIRC?
Dick
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For my commercial vessel batch I got good results but as my process is a bit different I don't think we should use this as a example . I may be getting a 200L reactor in a week so will be able to do batch size tests using traditional methods.
Paul
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has anyone done a batch yet and removed the acetone/meth from the batch straight away? maybe the acetone keeps reacting with the bio after the glys has been dropped but before the acetone/meth has been removed.
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has anyone done a batch yet and removed the acetone/meth from the batch straight away?
Yes me, went straight into condensing .
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has anyone done a batch yet and removed the acetone/meth from the batch straight away? maybe the acetone keeps reacting with the bio after the glys has been dropped but before the acetone/meth has been removed.
Me as well. Reacted till pass then demeth.
Some more pics
(http://i1279.photobucket.com/albums/y521/dickjotec/22bdf178b69955104f8963041c3e430d_zps67210c08.jpg)
From left
50/50 water and the foam. Kept in hot bunker 40C for 24 hours.
The foam after heating to 50C and cooled.
Sample from bottom output from settling tank taken after 4 days settling.
Sample from top of tank taken after 4 days settling.
All samples have had time to settle in the jars.
A sample from the top takeoff of the settling tank showed no fallout after several hours. Just doing a 50/50 on the sample.
The bio looks clear and has no floaters in it. The white band in the jar is interesting. Judging by the water at the bottom of the jar the foam must have had soap in it. I will post the results of the 50/50 later. This has split with no soap and a clear interface ATM I will leave till tomorrow then post pic.
Any ideas?
I will update the other thread with pics when I have them all done.
Dick
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So it's looking like the acetone reactions are are going to lend themselves to titrated acid water washing,
maybe with two or more acetone washes.
May not be the dogs danglies as we thought.
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So it's looking like the acetone reactions are are going to lend themselves to titrated acid water washing,
maybe with two or more acetone washes.
May not be the dogs danglies as we thought.
That was my thought initially after this batch but as I usually settle for 2+ weeks and it is already clear to the top takeoff I now think it might be OK.
I will certainly try again with less acetone and a WBD
Dick
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I have fuged out a fair amount of wax/HMPE's. from my batch over the last few cold days.
The top of my batch looks sparkling, the bottom is cloudy. The same as Dick's. Today with Paul we tested the cloudy Bio, it does not have any soap, it is PH neutral, it does not have any Methanol, Acetone or water in it !
It clears at 45c and goes cloudy again at 20c. Paul spun it up to 4000 rpm in his lab centrifuge and it came out cloudy the same as it went in.
I am thinking on the basis of what we tested today it would not do any harm to run it, I am fairly certain it would not cause problems with filters or anything else for that matter yet it would go against the grain !
Either I am going to pump it through the polishing pots when I next get to it on Thursday into my delivery tank and draw a few litres from the bottom of that tank after a couple of days and see what gives. Or I am going to take the cloudy fuel and try washing that on it's own, maybe with some acetone in the first wash !
Thoughts anyone ?
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Sounds exactly like mine. If it is HMPE then it would block filters so how about running it through a 1mic filter if you have one? Unfortunately I only go down to 5mic.
I intend to leave mine for 10 days. Then see what the bottom is like.
If you have any old bio from non acetone batch try adding acetone and see what happens?
Dick
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The only thing that worries me about washing it possable loss of yield.
Try it on some small samples first to see how you get on.
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Sounds exactly like mine. If it is HMPE then it would block filters so how about running it through a 1mic filter if you have one? Unfortunately I only go down to 5mic.
I intend to leave mine for 10 days. Then see what the bottom is like.
If you have any old bio from non acetone batch try adding acetone and see what happens?
Dick
It goes through a pair of 3 mic polishing pots on the way to my delivery tank then another polishing pot on the way to the car so I wont be worrying about the cars filter, however I do always carry a spare and the tools needed !
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The only thing that worries me about washing it possable loss of yield.
Try it on some small samples first to see how you get on.
Will do Mark. ;)
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Sounds exactly like mine. If it is HMPE then it would block filters so how about running it through a 1mic filter if you have one? Unfortunately I only go down to 5mic.
I intend to leave mine for 10 days. Then see what the bottom is like.
If you have any old bio from non acetone batch try adding acetone and see what happens?
Dick
It goes through a pair of 3 mic polishing pots on the way to my delivery tank then another polishing pot on the way to the car so I wont be worrying about the cars filter, however I do always carry a spare and the tools needed !
I wasn't thinking about the car filter rather if the cloudiness remains after filtering. If it does then I think we could be looking at something other than the HMPEs we know. Can you post the result after each pot?
Dick
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[/quote]
Can you post the result after each pot?
Dick
[/quote]
Unfortunately not it is all plumbed in.
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Decided to try it through the twin polishing pots, came out the other side in the clear pipe sparkling, the pressure at the pots did not increase from start to finish. That will do for this batch.
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Sounds good. If it did filter the HMPEs out there could not have been much else the pots would have blocked. I wonder if the effect of the acetone makes a small amount of HMPE look more?
I have filtered the white part of the jar water wash I did and think it is an emulsion made worse by the effect of the acetone. I will test it tomorrow.
I am quite happy with the result of using acetone and intend to do another batch to, hopefully improve the results.
Dick
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I had a 50/50 sample that had a middle layer exactly like yours, after fuging a couple of times the 50/50 was totally clear. I don't doubt though that it could be Acetone related as I had never seen anything like it before. Having said that I have gone months in between 50/50 testing so I could have missed a batch that reacted the same.
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My next batch is going to have more Acetone and less heat, how much of each I am yet to decide !
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I intend to react at same temp and reduce the acetone. Between us we may reach a conclusion about what is happening!
Dick
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Took sample from bottom take off in settling tank today now crystal clear and good 50/50, it will be at least another week before I filter into storage so it looks like a good result.
Dick
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Took sample from bottom take off in settling tank today now crystal clear and good 50/50, it will be at least another week before I filter into storage so it looks like a good result.
Dick
That's good to hear Dick.
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Based on their specific weights at 20*C
1 litre of Acetone would weigh 784.58g
1 litre of Methanol would weigh 787.73g
Additional weight for Methanol is 3.15g per litre.
So if for example 1 litre condensed distillate recovered after processing weighs say 785.30g
This would mean an additional 0.72g over the expected weight of just Acetone.
So by working out the percentage of the additional amount we can work out the volume of methanol.
eg. 0.72 divided by 3.15 = 0.2286
To get a percentage we times by 100
0.2286x100 = 22.86% and since we used 1 litre as a starting point
22.86% of 1 litre is 228.6 ml of Methanol
So we can then use this in the next batch, knowing how much Meth and how much Acetone we have in the distillate we can work out the volumes required.
I think this is right but please correct me if I am wrong I am not a chemist or mathematician! :-\
Just a quick one
Also in the distillate will be a % of water so not sure how accurate a sg test would be.
I could do a water in oil test but using a meth/water / acertone to see if I can get a accurate water result then do some simple sg test to see how well the calc's work out.
I'm affraid this my be a test for another day
Still pursuing this side of things :)
If the distillate is run through a 3A molecular sieve the water could be removed pretty much completely, so then we would be able to weigh a litre and know exactly what percentage of Acetone/Methanol there is.
We can then add whatever one is needed to bring it back to its right percentages.
I have done a lot of reading on these things and have basically come full circle back again to this conclusion. :-\
I cant contribute practical experience at the moment only theory but will try this when I am able to by mixing them and measuring.
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Sorry Dave I'm up to my neck in it at the moment ( haven't got time to swing a cat at mo) will try and do some test next week
Paul
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Sorry Dave I'm up to my neck in it at the moment ( haven't got time to swing a cat at mo) will try and do some test next week
Paul
Thats ok I wasn't rattling your cage ;D Im just getting a bit frustrated cos I cant do anything physical at the moment >:( so just reading lots and talking really...
Dont usually have the time to do it, funnily enough when reading up on drying acetone and methanol the best places I found info was on forums discussing cocaine manufacture and magic mushrooms! :o
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Thats ok I wasn't rattling your cage ;D Im just getting a bit frustrated cos I cant do anything physical at the moment >:( so just reading lots and talking really...
Dont usually have the time to do it, funnily enough when reading up on drying acetone and methanol the best places I found info was on forums discussing cocaine manufacture and magic mushrooms! :o
I saw a program on cocaine once, they were making it in drums not too dissimilar to ones we use for oil collection, but with with kerosene and diesel mixes and all sorts! All the waste hydrocarbon slurry just tipped into the jungle rivers. Yuk!
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Sorry Dave I'm up to my neck in it at the moment ( haven't got time to swing a cat at mo) will try and do some test next week
Paul
Thats ok I wasn't rattling your cage ;D Im just getting a bit frustrated cos I cant do anything physical at the moment >:( so just reading lots and talking really...
Dont usually have the time to do it, funnily enough when reading up on drying acetone and methanol the best places I found info was on forums discussing cocaine manufacture and magic mushrooms! :o
you noticed that as well? i got lots of stuff on making hash oil when i looked. not sure i would trust someone making hash oil to be totally precise in there measurements and conclusions. well they may have been when they started but as the product is being tested the measurements could start getting a little adrift. :-\
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you noticed that as well? i got lots of stuff on making hash oil when i looked. not sure i would trust someone making hash oil to be totally precise in there measurements and conclusions. well they may have been when they started but as the product is being tested the measurements could start getting a little adrift. :-\
Cannabis oil seems to be made with a bunch of stuff (Methanol, Isopropyl, Acetone - lots - whatever is available I guess) but we know that oils and Methanol don't mix. That said, maybe Cannabis plant oils are soluble in Methanol?
The idea of using harmful solvents for extraction doesn't strike me as a good idea, but if I was ever even thinking of possibly doing such a thing ::) Isopropyl would likely be best of a bad bunch.
Having not googled this extensively, what are the conclusions on the best way to dry solvents? I'm guessing fractional distillation is a little outside the realms of effort for most stoners.
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Having not googled this extensively, what are the conclusions on the best way to dry solvents? I'm guessing fractional distillation is a little outside the realms of effort for most stoners.
Was quite strange to read actually, these things being discussed on an open forum :(
Anyway what seemed to come up a lot was to use Epsom salts. The salts absorb water but not Acetone or Methanol, so you heat the salts to dry them first, then gradually add it to the Methanol, as it sucks up the water it forms into clumps so you keep adding it till it stops clumping, and stays as grains. It then drops down to the bottom of the jar and you just filter it out. Heat it to 150 degrees C to dry it then use it again.
The more scientific way is to use a Molecular sieve, basically crystals that are used in labs to dry these types of liquids. Good explanation here: http://www.bio.umass.edu/microscopy/mol_sieves.htm (http://www.bio.umass.edu/microscopy/mol_sieves.htm)
This is what I reckon we can use to dry our distillate to be able to work out volume of Methanol to Acetone
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not sure we want to be adding a possibly corrosive salt solution to our bio. i know molecular sieve no 3 is ok but not sure about epsom salts. does the water matter that much? apart from academically. we know the reaction works with less than 25% acetone so as long as we get most of the acetone back i cant see removing the water being too big a deal.
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I don't think the salt would remain in the meth/acetone , it would just settle to the bottom , I thing sodium sulphate would probable do the same job as this is another drying salt. For sodium sulphate I create about 100kg's a day just haven't got round to trying to dry it yet to see how good it is at water absorption. Is there a situation's vacant on this site I could do with a apprentice ( low wages harsh conditions grumpy boss )
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if you move down here i will be your apprentice. high wages clean working conditions and a day off to lie on the beach went the weather is fine,ohh and plenty of tea and biccys.
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I don't think the salt would remain in the meth/acetone , it would just settle to the bottom , I thing sodium sulphate would probable do the same job as this is another drying salt. For sodium sulphate I create about 100kg's a day just haven't got round to trying to dry it yet to see how good it is at water absorption. Is there a situation's vacant on this site I could do with a apprentice ( low wages harsh conditions grumpy boss )
If only you were closer!
Dick
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Is there a situation's vacant on this site I could do with a apprentice ( low wages harsh conditions grumpy boss )
When I was younger such a thing would have been more fun than work for me :)
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Anyway what seemed to come up a lot was to use Epsom salts. The salts absorb water but not Acetone or Methanol, so you heat the salts to dry them first, then gradually add it to the Methanol, as it sucks up the water it forms into clumps so you keep adding it till it stops clumping, and stays as grains. It then drops down to the bottom of the jar and you just filter it out. Heat it to 150 degrees C to dry it then use it again.
The more scientific way is to use a Molecular sieve, basically crystals that are used in labs to dry these types of liquids. Good explanation here: http://www.bio.umass.edu/microscopy/mol_sieves.htm (http://www.bio.umass.edu/microscopy/mol_sieves.htm)
This is what I reckon we can use to dry our distillate to be able to work out volume of Methanol to Acetone
That's very interesting.
With Acetone distillation at a much lower temp than water it would naturally favour distillate with only trace water - but as we know with Methanol it can easily lose purity with water present. This could solve that part of the Acetone cosolvent method.
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Was quite strange to read actually, these things being discussed on an open forum :(
Personally I think people should be entirely free to do whatever they like to themselves, so long as it doesn't harm others.
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Is there a situation's vacant on this site I could do with a apprentice ( low wages harsh conditions grumpy boss )
When I was younger such a thing would have been more fun than work for me :)
If you were any younger you'd still be one of those little swimming things.
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Is there a situation's vacant on this site I could do with a apprentice ( low wages harsh conditions grumpy boss )
When I was younger such a thing would have been more fun than work for me :)
If you were any younger you'd still be one of those little swimming things.
And kids should be seen but not heard, in anyway what's he doing down from the chimley.
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Is there a situation's vacant on this site I could do with a apprentice ( low wages harsh conditions grumpy boss )
When I was younger such a thing would have been more fun than work for me :)
If you were any younger you'd still be one of those little swimming things.
And kids should be seen but not heard, in anyway what's he doing down from the chimley.
Just fetching your teeth back grandpa, looks like they got carried up there on a sudden gust of hot air ;D
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not sure we want to be adding a possibly corrosive salt solution to our bio. i know molecular sieve no 3 is ok but not sure about epsom salts. does the water matter that much? apart from academically. we know the reaction works with less than 25% acetone so as long as we get most of the acetone back i cant see removing the water being too big a deal.
The salts don't dissolve into the acetone/meth but I was just saying what I read the molecular sieve is much better. The amount or removal of water is important because if you don't know the quantity in the distlate you cannot work out the volumes of acetone/methanol and therefore you can't work out what you are putting back into the next reaction
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Reading the molecular sieves info it occurs to me that it is for small amounts of water and solvent so while it will dry a sample for testing it would not be suitable for the amounts of liquid we would be using. The drying under vacuum of the used sieves would also be problematical.
Perhaps just testing a sample to establish the various proportions of constituents would be sufficient? Very accurate volume and weight measurements will be required.
Dick
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My bubblier was always in the very bottom, I'd have to pull it out of the settled soap/gly each time I did a new batch,
and then let it rest on top.
I've only ever seen honeycomb looking stuff form on top, and this was if I'd made a really soapy batch.
My bubbler is also resting on the last batches drop out and I never get a head like that in the picture. I did in the very early days of bio brewing but not for years now.
Just to add to this part of the debate, I've done an overdose batch (bone dry oil and excess catalyst) and got a single stage sparkling clear pass on the 5/45. Went on to do WBD up to 90C. Bubbled from 1/3 up from bottom of the settle drum this time, but still got a creamy/foamy top. So I don't think it is necessarily stirring up soaps from the bottom that causes it.
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Tony, I seem to remember having a conversation with you about this foam on top,
didn't we decide it was due to not demething completely.
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My bubblier was always in the very bottom, I'd have to pull it out of the settled soap/gly each time I did a new batch,
and then let it rest on top.
I've only ever seen honeycomb looking stuff form on top, and this was if I'd made a really soapy batch.
My bubbler is also resting on the last batches drop out and I never get a head like that in the picture. I did in the very early days of bio brewing but not for years now.
Just to add to this part of the debate, I've done an overdose batch (bone dry oil and excess catalyst) and got a single stage sparkling clear pass on the 5/45. Went on to do WBD up to 90C. Bubbled from 1/3 up from bottom of the settle drum this time, but still got a creamy/foamy top. So I don't think it is necessarily stirring up soaps from the bottom that causes it.
Was Acetone added to this batch ?
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Tony, I seem to remember having a conversation with you about this foam on top,
didn't we decide it was due to not demething completely.
It seems (though it's hard to tell) that there is a correlation between the amount of Methanol remaining and the time taken for this foam to appear when bubbling. So if I have a really well WBD'd batch it can appear in less than 24h, but otherwise it can take a couple of days of bubbling.
My feeling was that the foam appearing indicated that very little Methanol remained in the batch, so I bubble until I see it these days.
I suppose I should see if the foam is soluble in Methanol. I anticipate that it will be, certainly from conversations here it appears to be one and the same with the HMPE (or whatever it is) cream that forms at the bottom of batches. Usually I stir the foam into the surface and it sinks (to become "HMPE"s?)
Certainly from my reprocess batch the creamy stuff gives a 3/27 pass - soluble in Methanol - so if the foam is the same it will also be soluble in Methanol - which ties in with my speculation that it doesn't start to appear until the Methanol has been driven out.
My bubblier was always in the very bottom, I'd have to pull it out of the settled soap/gly each time I did a new batch,
and then let it rest on top.
I've only ever seen honeycomb looking stuff form on top, and this was if I'd made a really soapy batch.
My bubbler is also resting on the last batches drop out and I never get a head like that in the picture. I did in the very early days of bio brewing but not for years now.
Just to add to this part of the debate, I've done an overdose batch (bone dry oil and excess catalyst) and got a single stage sparkling clear pass on the 5/45. Went on to do WBD up to 90C. Bubbled from 1/3 up from bottom of the settle drum this time, but still got a creamy/foamy top. So I don't think it is necessarily stirring up soaps from the bottom that causes it.
Was Acetone added to this batch ?
No acetone in that one, no.
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I haven't been following this frothing issue word for word, so sorry if I've missed anything and the following is complete drivel. But if it only occurs when bubbling, could the issue be moist air, the same problem as I suspect I had when trying to dry oil and distill Methanol?
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It's certainly possible, when I did the 'foam' batch the air was very humid and cold. It may be the reason the 'HMPEs' foam but not why they form.
Dick
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It's certainly possible, when I did the 'foam' batch the air was very humid and cold. It may be the reason the 'HMPEs' foam but not why they form.
Dick
Our best guess about the so-called HMPE's is that they are really mono's or fats, so regardless of the conditions that cause them to form, they are better when they become apparent and are removed.
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It's certainly possible, when I did the 'foam' batch the air was very humid and cold. It may be the reason the 'HMPEs' foam but not why they form.
Dick
Our best guess about the so-called HMPE's is that they are really mono's or fats, so regardless of the conditions that cause them to form, they are better when they become apparent and are removed.
Personally I would rather know why they form and so not create them but I don't think the 'foaming' is a reliable indicator that they are present. In the past I have had more to remove and no foam on bubbling but of course this batch is the first I have done using acetone.
Dick
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It's certainly possible, when I did the 'foam' batch the air was very humid and cold. It may be the reason the 'HMPEs' foam but not why they form.
Dick
Our best guess about the so-called HMPE's is that they are really mono's or fats, so regardless of the conditions that cause them to form, they are better when they become apparent and are removed.
Personally I would rather know why they form and so not create them but I don't think the 'foaming' is a reliable indicator that they are present. In the past I have had more to remove and no foam on bubbling but of course this batch is the first I have done using acetone.
Dick
I totally agree ref the foam not being an indicator as I've never seen it. The point that I make about the 'HMPEs' is that there presence, assuming that they might be mono's or fats, means that you want them to form and then to get rid of them. So I guess you are right about the importance of know how they form, but it would be so that you could encourage them to form and then extract them.
Still theoretical, but if we're right, making them form should be part of the process unless the fats can be removed prior to reaction or if mono's, they can be prevented from forming in the reaction.
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I don't think so Julian, in the past when I've de-methed to the extream I've had foam forming as it's pumped into the settling drum,
this is not the normal bubbly foam that that disperses in a few mins, but sticky toffee type stuff that's still there days later.
I used to scoop it off the top with a child's fishing net.
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I think what we really need to try to find out is what 'they' are. Any ideas how we can test for the three possibles we have so far, HMPE, mono or fat? Has anyone got any other ideas to add to the three?
Dick
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I think what we really need to try to find out is what 'they' are. Any ideas how we can test for the three possibles we have so far, HMPE, mono or fat? Has anyone got any other ideas to add to the three?
Dick
Am I right in saying if they are mono or di then they should not pass a 90/10, I seem to recall Tony saying his passed !
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Am I right in saying if they are mono or di then they should not pass a 90/10, I seem to recall Tony saying his passed !
To the best of my knowledge its mono/di-glycerides that make a 10/90 cloudy yet show next to or nothing in drop out.
Anything less than a crystal clear 10/90 from the first to last drop of the 10ml bio sample indicates an incomplete reaction.
Mr GL said using deionized/distilled water in a 50/50 soap test will exposed mono's and di's as a creamy/white layer between the bio and water.
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Well let me add this into the mix. I found the photo I took of the batch I did with 45l "HMPEs" and 80l WVO.
This is a 10/100 test with the resulting mix before reaction:
(https://lh3.googleusercontent.com/-6r_KeGkPx_I/UQ_wwqtZYDI/AAAAAAAABI8/ofA5pECk2KQ/s512/IMG_20130108_230335.jpg)
6.4/10 (dropout/sample size) = 80/125 (WVO/batch size).
It is cloudy on top, but I put this down to something in the WVO - perhaps actually it was the "HMPEs" or - as we now suspect - monoglycerides.
That might also explain why reprocessing worked so well - I must've converted all the monos to FAMEs.
I've also tried water washing a sample of HMPEs before and that just made a right mayo mess, even with heat there was always a large white middle band and the water a brown tinted colour.
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OK let's assume for the moment they are mono and/or di glycs. We know they drop out of cold bio. They are indicated by a cloudy 10/90.
We need to know if they are caused by an incomplete reaction or a reverse reaction on demething.
How about this for a test?
Take a sample while reacting at the 10/90 pass and chill it in the deep freeze. If fallout is present continue to react till no falout then test again during and after demething.
Then do the same with an acetone batch and see if it is any different.
We should then know when they are forming and perhaps the cause.
Dick
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OK let's assume for the moment they are mono and/or di glycs. We know they drop out of cold bio. They are indicated by a cloudy 10/90.
We need to know if they are caused by an incomplete reaction or a reverse reaction on demething.
How about this for a test?
Take a sample while reacting at the 10/90 pass and chill it in the deep freeze. If fallout is present continue to react till no falout then test again during and after demething.
Then do the same with an acetone batch and see if it is any different.
We should then know when they are forming and perhaps the cause.
Dick
I think it will be difficult to test while reacting as I think it will not act the same when chilled until the Meth is out !
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As a matter of interest, mon and di-glycerides are used as emulsifiers in the food industry.
From my experience the glycerides only seem to precipitate out in the presents of water, incomplete reaction leaves mono and di's suspended in the bio, water was and hey presto.
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OK let's assume for the moment they are mono and/or di glycs. We know they drop out of cold bio. They are indicated by a cloudy 10/90.
We need to know if they are caused by an incomplete reaction or a reverse reaction on demething.
How about this for a test?
Take a sample while reacting at the 10/90 pass and chill it in the deep freeze. If fallout is present continue to react till no falout then test again during and after demething.
Then do the same with an acetone batch and see if it is any different.
We should then know when they are forming and perhaps the cause.
Dick
I think it will be difficult to test while reacting as I think it will not act the same when chilled until the Meth is out !
Good point. Back to the drawing board.
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As a matter of interest, mon and di-glycerides are used as emulsifiers in the food industry.
From my experience the glycerides only seem to precipitate out in the presents of water, incomplete reaction leaves mono and di's suspended in the bio, water was and hey presto.
This could point to bubbling with damp air bringing them up? Perhaps it would be worth drying the air some how?
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As a matter of interest, mon and di-glycerides are used as emulsifiers in the food industry.
From my experience the glycerides only seem to precipitate out in the presents of water, incomplete reaction leaves mono and di's suspended in the bio, water was and hey presto.
This could point to bubbling with damp air bringing them up? Perhaps it would be worth drying the air some how?
Never had a cloudy 10/90 pass at 20 deg C, don't bubble, do water wash until a 50/50 clear, but it still drops out at sub-zero temps. So probably nothing to do with bubbling.
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As a matter of interest, mon and di-glycerides are used as emulsifiers in the food industry.
From my experience the glycerides only seem to precipitate out in the presents of water, incomplete reaction leaves mono and di's suspended in the bio, water was and hey presto.
But we only see it in winter - and the rest of the bio is crystal clear. It could be that the monos have a higher melt point than bio but we don't see them in summer because of the heat.
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As a matter of interest, mon and di-glycerides are used as emulsifiers in the food industry.
From my experience the glycerides only seem to precipitate out in the presents of water, incomplete reaction leaves mono and di's suspended in the bio, water was and hey presto.
This could point to bubbling with damp air bringing them up? Perhaps it would be worth drying the air some how?
Never had a cloudy 10/90 pass at 20 deg C, don't bubble, do water wash until a 50/50 clear, but it still drops out at sub-zero temps. So probably nothing to do with bubbling.
I was thinking of the foam that formed on the top of my acetone batch. I have never had foam before and I don't think bubbling causes the monos just brings them up if the air is damp?
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Ah! Can't play with the new chems at the mo :'(
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I am going to do another acetone batch tomorrow. 160L stage 1 25l meth 800 NaOH 400ml acetone. I will finalise the pics of the 'HMPE' and update the. Other thread hopefully tomorrow.
We could really do with a name for the HMPE/ mono / di gly/ fats until we know what they are (if we ever do!) Fallout does not seem to fit the purpose.
Dick
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I am going to do another acetone batch tomorrow. 160L stage 1 25l meth 800 NaOH 400ml acetone. I will finalise the pics of the 'HMPE' and update the. Other thread hopefully tomorrow.
We could really do with a name for the HMPE/ mono / di gly/ fats until we know what they are (if we ever do!) Fallout does not seem to fit the purpose.
Dick
Well the HMP is correct, we just don't know if they are esters, perhaps HMPC. ! !
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Ps: good luck with the batch.
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I have filtered the HMP? from the last batch out through a sheet. This is the residue, around 5L but I have not measured it yet.
(http://i1279.photobucket.com/albums/y521/dickjotec/5a156f76ab92a59dbcb37a51012ad1bd_zps8105f192.jpg)
The new batch is going fine.
160L
800g NaOH
25L meth
400ml acetone
Fall out 2
5L
160g
Pass
After stage 1 about half the usual amount of glyc.
Now heating to WBD
Dick
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I have filtered the HMP? from the last batch out through a sheet. This is the residue, around 5L but I have not measured it yet.
(http://i1279.photobucket.com/albums/y521/dickjotec/5a156f76ab92a59dbcb37a51012ad1bd_zps8105f192.jpg)
The new batch is going fine.
160L
800g NaOH
25L meth
400ml acetone
Fall out 2
5L
160g
Pass
After stage 1 about half the usual amount of glyc.
Now heating to WBD
Dick
Could you see the high melting point elements before filtering? I recon my settled out in the cold fuel would go straight through a sheet etc. as it looks good and clear prior to filtering.
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I have filtered the HMP? from the last batch out through a sheet. This is the residue, around 5L but I have not measured it yet.
(http://i1279.photobucket.com/albums/y521/dickjotec/5a156f76ab92a59dbcb37a51012ad1bd_zps8105f192.jpg)
The new batch is going fine.
160L
800g NaOH
25L meth
400ml acetone
Fall out 2
5L
160g
Pass
After stage 1 about half the usual amount of glyc.
Now heating to WBD
Dick
That seems a lot from 1 batch, what was your feedstock again ? what temperature was this filtering done at ?
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It was not all from the one batch so I can't say how much of it was the acetone batch, I last emptied the tank a couple of months, or more, ago. Feedstock is mixed runny oil, not much whites in the last batch, or this one.
It was filtered at ambient over a period of days. Temps here have been around freezing.
I will know better with this batch as the tank is now clean.
Dick
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I have filtered the HMP? from the last batch out through a sheet. This is the residue, around 5L but I have not measured it yet.
The new batch is going fine.
160L
800g NaOH
25L meth
400ml acetone
Fall out 2
5L
160g
Pass
After stage 1 about half the usual amount of glyc.
Now heating to WBD
Dick
Could you see the high melting point elements before filtering? I recon my settled out in the cold fuel would go straight through a sheet etc. as it looks good and clear prior to filtering.
Yes it was very obvious, I took about 25l of bio out of the bottom of the tank and put it throug the sheet. The bio that went through now looks clear.
Dick
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With that amount of HMPE I reckon you should drop the WBD for the next batch and only demeth the Bio, I stop WBD when winter arrives to prevent exactly that problem.
You can always recover most of the methanol in the glyc with a glyc wash.
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With that amount of HMPE I reckon you should drop the WBD for the next batch and only demeth the Bio, I stop WBD when winter arrives to prevent exactly that problem.
You can always recover most of the methanol in the glyc with a glyc wash.
That was a bio only demeth! As said above it was probably not from just the acetone batch.
I am just settling the next acetone batch. This is WBD but interestingly I have got no more meth back than in the last batch.
Will post results after I have decanted in an hour.
Dick
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Brief results from 160L acetone 400ml batch.
Condensate. 7L
Glyc. 25L
Bio. 157L
These are approximate. It is now bubbling will it foam again?
Very pleased less glyc more bio than normal 2 stage for me.
Dick
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Hi,
I am very new to this board and very new to biodiesel production. I just want to thank you all for the work that you are doing.
Right now I am doing a lot of research and reading because I have a bit of time on my hands.
I'm reading the Biodiesel Handbook by Gerhard Knothe and Jon Van Gerpen. In the chapter concerning transesterification it talks about glycerin removal. It also lists that alcohols can be used to keep glycerin soluble in biodiesel. I believe I read earlier that less glycerin is being removed from the reactor with acetone assisted reactions. Could the glycerin be dissolved in the biodiesel? Wouldn't this adversely effect the amount of free glycerol and total glycerol in the end product? I only ask because measuring glycerol content in the biodiesel is an ASTM and EN quality standard.
For the homebrewer this might not be a major concern but, having those long chain hydrocarbons passing through your engine cannot be a good thing.
Sorry to interupt but I thought this would be a great place to ask my questions.
Thanks
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I'd be surprised if the glyc is simply in solution with the bio. The acetone co-solvent process was pioneered by an academic institution and the final product was tested to ASTM standards.
Some brewers tested here have been doing it in conjunction with water washing, which ought to flush any glycerin out. But you are right having glycerin present in the final product isn't a good idea:
http://www.biopowered.co.uk/wiki/Effect_of_biodiesel_on_fuel_injection_systems (http://www.biopowered.co.uk/wiki/Effect_of_biodiesel_on_fuel_injection_systems)
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Hi,
I am very new to this board and very new to biodiesel production. I just want to thank you all for the work that you are doing.
Right now I am doing a lot of research and reading because I have a bit of time on my hands.
I'm reading the Biodiesel Handbook by Gerhard Knothe and Jon Van Gerpen. In the chapter concerning transesterification it talks about glycerin removal. It also lists that alcohols can be used to keep glycerin soluble in biodiesel. I believe I read earlier that less glycerin is being removed from the reactor with acetone assisted reactions. Could the glycerin be dissolved in the biodiesel? Wouldn't this adversely effect the amount of free glycerol and total glycerol in the end product? I only ask because measuring glycerol content in the biodiesel is an ASTM and EN quality standard.
For the homebrewer this might not be a major concern but, having those long chain hydrocarbons passing through your engine cannot be a good thing.
Sorry to interupt but I thought this would be a great place to ask my questions.
Thanks
Hi JV3, welcome to the forum.
Always good to have another persons input, clearly you are doing lots of reading, keep it up and keep asking questions. In the midst of it sometimes we can see things with clouded vision.
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Hi,
I am very new to this board and very new to biodiesel production. I just want to thank you all for the work that you are doing.
Right now I am doing a lot of research and reading because I have a bit of time on my hands.
I'm reading the Biodiesel Handbook by Gerhard Knothe and Jon Van Gerpen. In the chapter concerning transesterification it talks about glycerin removal. It also lists that alcohols can be used to keep glycerin soluble in biodiesel. I believe I read earlier that less glycerin is being removed from the reactor with acetone assisted reactions. Could the glycerin be dissolved in the biodiesel? Wouldn't this adversely effect the amount of free glycerol and total glycerol in the end product? I only ask because measuring glycerol content in the biodiesel is an ASTM and EN quality standard.
For the homebrewer this might not be a major concern but, having those long chain hydrocarbons passing through your engine cannot be a good thing.
Sorry to interupt but I thought this would be a great place to ask my questions.
Thanks
Hi JV3, welcome to the forum.
Always good to have another persons input, clearly you are doing lots of reading, keep it up and keep asking questions. In the midst of it sometimes we can see things with clouded vision.
[/quothi jv3 and welcome to the forum,
i think what is happening is that more oil is being converted to bio than in the other methods. this will result in less bio being trapped in the glyserol so the yeald will go up at the expense of glyserol. comparing the 2 this would show as less glyserol. this is only a theory as i have not done any tests yet.
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If someone who is doing a acetone reaction wants me to do some tests on their Glyc to see if it is a case of more oils and FFA's are reacted and not left behind in the Glyc.
Paul
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having those long chain hydrocarbons passing through your engine cannot be a good thing.
I was under the impression that those long chain hydrocarbons are the fuel,
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having those long chain hydrocarbons passing through your engine cannot be a good thing.
I was under the impression that those long chain hydrocarbons are the fuel,
Yar, indeed they are, be that fatty acids, FAME, monoglycerides... I think JV3 means the Glycerol molecule ripped from the middle of the triglyceride. Don't want that in the fuel, that's for sure :) But as said above water washing takes care of it because it's soluble in water whereas FAME is not.
At least the 50:50 water test will still show it so there is an indication of quality even with fuel that is just gravity settled.
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If someone who is doing a acetone reaction wants me to do some tests on their Glyc to see if it is a case of more oils and FFA's are reacted and not left behind in the Glyc.
Paul
I have the glyc from the last acetone batch. It was WBD. How much do you need for testing?
Pm me your address and I will send it over.
Regarding that batch I have a very small amount of foam on this one and a sample from the bottom takeoff on the settling tank is already clear. Have not 50/50 tested it yet as it was only made on Sunday evening.
Will post results and pics later in week.
Dick
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Cheers dick
I'm getting some from Steve soon , if the test is a success then I will get you to send a sample down I will send you my home address as I don't always get mail at unit.
Paul
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Cheers dick
I'm getting some from Steve soon , if the test is a success then I will get you to send a sample down I will send you my home address as I don't always get mail at unit.
Paul
Paul did you get my email about the acid.?
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Hi bob
Yes got your email
I will try and get some out to everone over the next few days.
Paul
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thanks paul, sorry to highjack the thread. keep calm and drink tea, and dunk biscuits.